US1817968A - Preparation of adsorbents - Google Patents

Description

Patented Aug. 11, 1931 I UNITED STATES PATENT OFFICE ROY CROSS, OF KANSAS CITY, MISSOURI, ASSIGNOR '10 CROSS DEVELOPMENT CORPORA- TION, A CORPORATION OF DELAWARE PREPARATION OF .ADSORBENTS No Drawing. Original application filed December 22, 1921, Serial No. 524,290. Divided and this application filed November 10, 1923. Serial No 674,043.

This application is a divisional of an original application, SerialNo. 524,290, filed under date of December 22nd, 1921.

My invention relates to a method of treating hydrocarbons and has for its object the dehydration, decolorization and neutralization of oil'by the intimate contacting of theoil either in the liquid or vapor state with dried hydrous silicate of alumina. The most valuable hydrous silicate of alumina or Zeolite for this purpose is the-- naturally occurring substance known as Bentonite. Bentonite is the best of this class of adsorbent material and is possibly the active principle to be found in fullers earth. A typical quality of Bentonite is that. found near Ardmore, South Dakota, and has the following composition:

This material has the property of absorb ing a very large amount of water, forming a gelatinous mass with it and is capable of being diluted with water and forming a colloid to such a degree that the water permanently remains milky.

For the purpose of use, the hydrous silicate of alumina is perfectly dried but not ignited. It is then crushed and screened to the sizes desired. For some purposes it is used in a finely divided powder, others as coarse granules. For the dehydration of oils, the coarse granules are best as they absorb the water from the oil without producing a turbidity. For decolorizing lubricating oils, the coarse granules are best as they form a bed more pervious to the passage of the oil. To obtain the greatest de-v colorizing action, however, the more finely,

passing dry chlorine over the hot hydrous silicate of alumina. This renews the absorptive effect of the hydrous silicate of alumina and in addition, forms a small amount of anhydrous aluminum chloride, because of the chemical susceptibility of the aluminum silicate in this form.

When rejuvenated by chlorine, however, the hydrous silicate of alumina must be kept in perfectly dry.containers.-

The method of applying the hydrous silicate of alumina to the oil depends upon the character of the oil to be treated. In the case of pressure benzine or gasoline such as is obtained in the ordinary cracking plant, the color of the gasoline is such that it cannot be marketed under the ordinar Navy specifications. Decolorization is e fected by pumping the gasoline through a warm bed of hydrous silicate of alumina and discharging ,it into a still containing hydrous silicate of alumina. The vapors arising from the still are made to pass and the amount of hydrous silicate of alumina required varies with the character of the distillate. Ordinarily when rocesses such as the Cross process, described in Patent No. 1,423,500, are used, one pound of hydrous silicate of alumina in finely divided condition is suflicient for one pound of gasoline.

If the hydrous silicate of alumina is placed in the still ,alone a larger quantity is required. When distillation is complete, the

hydrous silicate of alumina is steamed out to remove all of the oil and the particles have a greenish to black appearance. The used hydrous silicate of alumina is now placed in the ordinary fullers earth burners -'in which the volatile carbonaceous matter is removed. From the fullers earth burner it is discharged into a vertical tile tower through which is passed a current of dry chlorine gas at such a rate and in such quantity that the chlorine gas does not appreciably escape from the top. The residue at the bottom'is drawn OE and again used. When the residue after treatment with chlorine is used, it has been found that the gasoline distilled has a' lower end point and a lower content of olefin compounds and the odor of the gasoline is considerably improved.

In the dehydration of petroleum, the petroleum only has to pass through the granular hydrous silicate of alumina toremove the water. In this case, the hydrous silicate of alumina is regenerated merely by heating to drive off the moisture until it becomes so impregnated with carbonaceous matter that it issubjected to the treatment herein described for revivifying the exhausted material.

ing the material, and subjecting the treated material to the action of dry chlorine gas, as and for the purpose described.

5. A process for revivifying and modifying the character of spent bentonite resulting from the treatment of oils with bentonite, which comprises driving ofl:' adsorbedv volatile carbonaceous substances retained in the spent bentonite, and thereafter treating the bentonite with chlorine gas.

ROY GRUSS.

In the treatment of kerosene or other refined petroleum, which has previously been treated with acid, the hydrous silicate of alumina removes the last trace of acid as well as decolorizes and dehydrates the oil.

The treatment of lubricants with hydrous silicate of alumina is accomplished in the same manner as with ordinary fullers earth using preferably 20. to 30 mesh material. 'Ihe residual hydrous silicate of alumina is regenerated in the usual manner except that the added step of treatment with dry chlorine is used.

For the treatment of transformer oils, hydrous silicate of alumina is particularly valuable as it removes the last trace of moisture without adding anything to the oil which will have a greater conductivity than the water even in case thelast traces of hydrous silicate of alumina are not removed.

I claim as my invention:

1. A process for the revivification and treatment of'bentonite for use in refining 011, comprising passing dry chlorine; gas in contact therewith at temperatures sufficiently high to effect a combination of the chlorine and alumina constituents.

2. A process for the revivification and treatment of bentonite for use in oil refining, comprising the steps of initially heatmg the material, and passing dry chlorine gas thereover sufiiciently heated to efiect a combination of the chlorine and alumina constitutents. p

3. A process for the revivification and treatment of bentonite, comprising initially